Process And Apparatus For Producing Powder Particles By Atomization Of A Feed Material In The Form Of An Elongated Member

ABSTRACT

The present disclosure relates to a process and an apparatus for producing powder particles by atomization of a feed material in the form of an elongated member such as a wire, a rod or a filled tube. The feed material is introduced in a plasma torch. A forward portion of the feed material is moved from the plasma torch into an atomization nozzle of the plasma torch. A forward end of the feed material is surface melted by exposure to one or more plasma jets formed in the atomization nozzle. The one or more plasma jets being includes an annular plasma jet, a plurality of converging plasma jets, or a combination of an annular plasma jet with a plurality of converging plasma jets. Powder particles obtained using the process and apparatus are also described.

CROSS REFERENCE TO RELATED APPLICATIONS

This application is a continuation of International Application No.PCT/CA2015/050174, filed on Mar. 9, 2015, which claims priority to andbenefit of U.S. Provisional Application No. 61/950,915, filed on Mar.11, 2014 and U.S. Provisional Application No. 62/076,150, filed on Nov.6, 2014, the entire disclosures of each of which are hereby incorporatedby reference.

TECHNICAL FIELD

The present disclosure relates to the field of materials processing.More specifically, the present disclosure relates to a process and to anapparatus for producing powder particles by atomization of a feedmaterial in the form of an elongated member. Powder particles producedusing the disclosed process and apparatus are also disclosed.

BACKGROUND

With the growing interest in rapid prototyping and manufacturing,commonly known as additive manufacturing or 3-D printing, a number oftechniques have been developed for the production of dense sphericalpowders, which are useful for such technologies. The success of additivemanufacturing and 3-D printing depends in a large extent on theavailability of materials usable for parts manufacturing. Such materialsneed to be provided in the form of highly pure, fine (e.g. diameter lessthan 150 μm), dense, spherical, and free-flowing powders that havewell-defined particle size distributions. Conventional melt atomizationtechniques such as gas, liquid and rotating disc atomization are unableto produce such high quality powders.

More recent techniques avoid the use of crucible melting, which is oftenresponsible for material contamination. These recent techniques providespherical, free-flowing powders.

For example, some plasma atomization processes are based on the use of aplurality of plasma torches producing plasma jets that converge towardan apex. By feeding a material to be atomized in the form of a wire orrod into the apex, the material is melted and atomized by thermal andkinetic energy provided by the plasma jets. It has also been proposed tofeed a material to be atomized in the form of a continuous molten streamdirected towards an apex where several plasma jets converge. These typesof plasma atomization processes are rather delicate and requirelaborious alignment of at least three plasma torches in order to have atleast three plasma jets converging toward the apex. Due to the physicalsize of such plasma torches, the apex location is bound to be a fewcentimeters away from an exit point of the plasma jets. This causes aloss of valuable thermal and kinetic energy of the plasma jets beforethey reach the apex position and impinge on the material. Overall, theseprocesses involve several difficulties in terms of requirements forprecise alignment and power adjustment of the torches and for precisesetting of the material feed rate.

Other technologies are based on the use of direct induction heating andmelting of a wire or rod of a material to be atomized while avoidingcontact between the melted material and a crucible. Melt droplets fromthe rod fall into a gas atomization nozzle system and are atomized usinga high flow rate of an appropriate inert gas. A main advantage of thesetechnologies lies in avoiding possible contamination of the material tobe atomized by eliminating any possible contact thereof with a ceramiccrucible. These technologies are however limited to the atomization ofpure metals or alloys. Also, these technologies are complex and requirefine adjustment of operating conditions for optimal performance.Furthermore, large amounts of inert atomizing gases are consumed.

Therefore, there is a need for techniques for efficient and economicalproduction of powder particles from a broad range of feed materials.

SUMMARY

According to a first aspect, the present disclosure relates to a processfor producing powder particles by atomization of a feed material in theform of an elongated member that includes introducing the feed materialin a plasma torch, moving a forward portion of the feed material fromthe plasma torch into an atomization nozzle of the plasma torch; andsurface melting a forward end of the feed material by exposure to one ormore plasma jets formed in the atomization nozzle, the one or moreplasma jets being selected from an annular plasma jet, a plurality ofconverging plasma jets, and a combination thereof.

According to another aspect, the present disclosure relates to anapparatus for producing powder particles by atomization of a feedmaterial in the form of an elongated member, comprising a plasma torchincluding: an injection probe for receiving the feed material; and anatomization nozzle configured to receive a forward portion of the feedmaterial from the injection probe, be supplied with plasma, produce oneor more plasma jets, and melt a surface of a forward end of the feedmaterial by exposure to the one or more plasma jets. The one or moreplasma jets are selected from an annular plasma jet, a plurality ofconverging plasma jets, and a combination thereof.

The foregoing and other features will become more apparent upon readingof the following non-restrictive description of illustrative embodimentsthereof, given by way of example only with reference to the accompanyingdrawings. Like numerals represent like features on the various figuresof drawings.

BRIEF DESCRIPTION OF THE DRAWINGS

Embodiments of the disclosure will be described by way of example onlywith reference to the accompanying drawings, in which:

FIG. 1 is a front elevation view of a plasma torch usable foratomization of feed material in the form of an elongated member such as,as non-limitative examples, a wire, rod or filled tube;

FIG. 2A is a detailed, front elevation view of the plasma torch of FIG.1 , having an atomization nozzle according to an embodiment and aconfiguration for direct preheating of the elongated member by theplasma;

FIG. 2B is a detailed, front elevation view of the plasma torch of FIG.1 , having the atomization nozzle of FIG. 2A and a configuration inwhich the elongated member is indirectly heated by the plasma through aradiation tube;

FIG. 3 is a front elevation view of an apparatus for atomization of feedmaterial in the form of an elongated member, the apparatus including theplasma torch of FIG. 1 ;

FIG. 4A is a perspective view of an atomization nozzle with a supportflange according to an embodiment;

FIG. 4B is a cross-sectional view of the atomization nozzle and supportflange of FIG. 4A;

FIG. 4C, FIG. 4D and FIG. 4E are additional top, bottom and perspectiveviews showing details of the atomization nozzle of FIG. 4A, including acentral aperture surrounded by radial apertures for producing plasmajets;

FIG. 5 is a detailed, front elevation view of the plasma torch of FIG. 1, showing an atomization nozzle according to another embodiment;

FIG. 6 is a detailed, front elevation view of a variant of the plasmatorch of FIG. 1 , showing the atomization nozzle of FIG. 5 and furtherincluding a sheath gas port surrounding the exit end of the atomizationnozzle;

FIG. 7 is a flow chart showing operations of a process of producingpowder particles by atomization of a feed material in the form of anelongated member such as, as non-limitative examples, a wire, rod orfilled tube;

FIG. 8 is a schematic view, including a graph showing modelling resultsfor heating a 3.2 mm stainless steel wire introduced in anargon/hydrogen induction plasma at 60 kW;

FIG. 9 is an electron micrograph of powder particles obtained byatomization of a 3.2 mm diameter stainless steel wire and a graph ofcorresponding particle size distribution; and

FIG. 10 illustrates electron micrographs of different stainless steelspherical powder fractions produced using the process and apparatus forproducing powder particles by atomization of a feed material in the formof an elongated member.

DETAILED DESCRIPTION

Generally speaking, the present disclosure addresses one or more of theproblems of efficiently and economically producing powder particles froma broad range of feed materials.

More particularly, the present disclosure describes a plasma atomizationprocess and an apparatus therefor, usable to produce powder particlesfrom a broad range of feed materials, including for example pure metals,alloys, ceramics and composites. The disclosed technology may be used inthe manufacture of a wide range of dense spherical metal, ceramic orcomposite powders from a feed material of the same nature in the form ofan elongated member such as, as non-limitative examples, a rod, a wireor a filled tube. A powder may be defined as comprising particles with adiameter of less than one (1) millimeter, a fine powder may be definedas comprising of particles of diameter less than 10 micrometers, whilean ultrafine powder may be defined as comprising particles of less thanone (1) micrometer in diameter.

In a non-limitative embodiment, the plasma torch, which may optionallybe an inductively coupled plasma torch, is supplied with the feedmaterial along a central, longitudinal axis thereof. A speed of movementand/or a distance of travel of the feed material in an optionalpreheating zone of the plasma torch may be controlled to allow thematerial to heat to a temperature as close as possible to its meltingpoint while avoiding premature melting thereof within the plasma torch.In one embodiment, a forward end of the optionally preheated feedmaterial enters the atomization nozzle to emerge from its downstreamside and enter a cooling chamber. Due to its passage in the atomizationnozzle, the forward end or tip of the feed material is exposed to aplurality of plasma jets, for example high velocity plasma jets,including, though not limited to, supersonic fine plasma jets. Uponimpinging on the feed material, the plasma jets melt its surface andstrip out molten material resulting in finely divided, spherical moltendroplets of the material entrained with the plasma gas from theatomization nozzle. In another embodiment, the forward end of theoptionally preheated feed material is exposed to an annular plasma jetwithin the atomization nozzle, the annular plasma jet also causingsurface melting of the feed material. Resulting droplets are entrainedby the plasma gas into the cooling chamber. In both embodiments, thedroplets cool down and freeze in-flight within the cooling chamber,forming for example small, solid and dense spherical powder particles.The powder particles can be recovered at the bottom of the cooingchamber, for example in a downstream cyclone or in a filter, dependingon their particle size distribution.

In the context of the present disclosure, powder particles obtainedusing the disclosed process and apparatus may include, withoutlimitation, micron sized particles that may be defined as particles in arange from 1 to 1000 micrometer in diameter.

The following terminology is used throughout the present disclosure:

-   -   Powder particle: a grain of particulate matter, including but        not limited to micron sized and nanoparticles.    -   Atomization: reduction of a material into particles.    -   Feed material: a material to be transformed by a process.    -   Filled tube: feed material provided in the form of a tube, made        as non-limitative examples of metal, plastic or any other        suitable material, filled with a powder composed of a pure        metal, alloys, ceramic material, any other suitable material, or        composed of a mixture of materials, so that melting the powder        can give rise to the formation of an alloy or composite    -   Plasma: a gas in a hot, partially ionized state.    -   Plasma torch: a device capable of turning a gas into plasma.    -   Inductively coupled plasma torch: a type of plasma torch using        electric current as an energy source to produce electromagnetic        induction of the energy into the plasma.    -   Injection probe: an elongated conduit that may be cooled using a        cooling fluid, for insertion or supply of a feed material.    -   Preheating zone: area in a plasma torch in which feed material        is elevated to a temperature below its melting point,    -   Atomization nozzle: element to produce plasma jets and to allow        feed material to transfer from a plasma torch to a cooling        chamber.    -   In-flight freezing: cooling of liquid droplets becoming solid        particles while suspended within a gas.    -   Cooling chamber a container in which in-flight freezing takes        place.

Referring now to the drawings, FIG. 1 is a front elevation view of aplasma torch usable for atomization of feed material in the form of anelongated member such as, as non-limitative examples, a wire, rod orfilled tube. Obviously, other types of elongated member couldpotentially be used in the disclosed process and apparatus foratomization of feed material.

FIG. 2A is a detailed, front elevation view of the plasma torch of FIG.1 , having an atomization nozzle according to an embodiment and aconfiguration for direct preheating of the elongated member by theplasma, while FIG. 2B is a detailed, front elevation view of the plasmatorch of FIG. 1 , having the atomization nozzle of FIG. 2A and aconfiguration in which the elongated member is indirectly heated by theplasma through a radiation tube. FIG. 3 is a front elevation view of anapparatus for atomization of feed material in the form of an elongatedmember, the apparatus including the plasma torch of FIG. 1 .

Referring at once to FIGS. 1, 2 and 3 , an apparatus 100 for producingpowder particles by atomization of a feed material 110 in the form of anelongated member such as, as non-limitative examples, a wire, a rod or afilled tube, comprises a plasma torch 120 producing plasma 126, and acooling chamber 170. Without limiting the present disclosure, the plasmatorch 120 as shown is an inductively coupled plasma torch. Use of othertypes of plasma torches is also contemplated. The apparatus 100 mayfurther comprise a powder collector 190.

The plasma torch 120 comprises an injection probe 122 in the form of anelongated conduit mounted onto the head 185 coaxial with the inductivelycoupled plasma torch 120. As illustrated in FIG. 1 , the injection probe122 extends through the head 185 and through the plasma confinement tube179. The feed material 110 can be inserted in the plasma torch 120 viathe injection probe 122 so that it is coaxial with the torch body 181.The feed material 110 may be supplied to the injection probe 122, incontinuous manner, by a typical wire, rod or tube feeding mechanism (notshown) for example similar to commercially available units currentlyused in wire arc welding such as the units commercialized by Miller forMIG/Wire welding, and comprising a first set of wheels operated tocontrol the feed rate of the elongated member to the injection probe122. The feeding mechanism may be either preceded or followed by twosuccessive sets of straightening wheels to straighten the elongatedmember within two perpendicular planes. Of course, in some situations,only one set or more of straightening wheels may be required tostraighten the elongated member within one plane only or multipleplanes. The set(s) of straightening wheels are useful when the feedmaterial is supplied under the form of rolls. In a variant, the feedingmechanism may be adapted to rotate the feed material 110 about alongitudinal axis thereof, specifically about a longitudinal axis of theplasma torch 120.

A preheating zone 124 for preheating a forward portion 112 of the feedmaterial 110, either by direct contact with the plasma 126 asillustrated in FIG. 2A or by radiation heating from a radiation tube 125surrounding the feed material 110, the radiation tube 125 itself beingheated by direct contact with the plasma 126, as illustrated in FIG. 28. The radiation tube 125 may be made, for example, of refractorymaterial such as graphite, tungsten or hafnium carbide. The plasma torch120 also comprises an atomization nozzle 160 with a channel throughwhich the forward portion 112 of the feed material 110 from thepreheating zone 124 travels to expose a forward end 114 of the feedmaterial 110 to a plurality of plasma jets 180 and atomize the feedmaterial. The channel may comprise a central aperture 162 allowing theforward portion 112 of the feed material 110 to exit the plasma torch120 and enter the cooling chamber 170, and with radial apertures 166 forproducing the plurality of plasma jets 180. The cooling chamber 170 ismounted to the lower end of the plasma torch 120, downstream of thenozzle 160. In the cooling chamber 170, the forward end 114 of the feedmaterial 110 is exposed to the plurality of plasma jets 180.

Still referring to FIGS. 1, 2 and 3 and although other types of plasmatorches could eventually be used, the plasma torch 120 is an inductivelycoupled plasma torch and comprises an outer cylindrical torch body 181,an inner cylindrical plasma confinement tube 179, and at least oneinduction coil 130 in a coaxial arrangement. The outer cylindrical torchbody 181 may be made of moldable composite material, for example amoldable composite ceramic material. The inner cylindrical plasmaconfinement tube 179 may be made of ceramic material and, as indicatedhereinabove, is coaxial with the torch body 181. The at least oneinduction coil 130 is coaxial with and embedded in the torch body 181 toproduce a RF (radio frequency) electromagnetic field whose energyignites and sustains the plasma 126 confined in the plasma confinementtube 179 including preheating zone 124. The plasma is produced from atleast one gas such as argon, helium, hydrogen, oxygen, nitrogen or acombination thereof, supplied within the plasma confinement tube 179through a head 185 of the inductively coupled plasma torch 120 at theupper end of the torch body 181. RF current is supplied to the inductioncoil(s) 130 via power leads 132. Water or another cooling fluid is fedvia inlets such as 134, flows in cooling channels such as 136, inparticular through an annular spacing between the torch body 181 and theplasma confinement tube 179, for cooling the inductively coupled plasmatorch. The water or other cooling fluid exits the apparatus 100 viaoutlets such as 138. Water or other cooling fluid may also flow (a)within a shield 140 of the injection probe 122 and into the inductioncoil(s) 130 which is (are) then tubular.

Exposure of the forward end 114 of the feed material 110 to theplurality of plasma jets 180 causes local melting of the feed materialfollowed by instantaneous stripping and breakdown of the formed moltenlayer of feed material into small droplets 182. The droplets 182 fallinto the cooling chamber 170, which is sized and configured to allowin-flight freezing of the droplets 182. The droplets 182, when freezing,turn into powder particles 184 collected in the collector 190.

The apparatus 100 of FIG. 3 is configured to let the droplets 182 falltowards the collector 190 by gravity. However, other configurations inwhich the droplets 182 do not fall vertically, being propelled by a gasor by a vacuum, are also contemplated. In the embodiment of FIG. 3 andin such other configurations, an exit pipe 192 may connect a lower partof the cooling chamber 170 toward a vacuum pumping system (not shown) towithdraw gas from the cooling chamber 170.

The apparatus 100 includes other components such as casings, flanges,bolts, and the like, which are illustrated on FIGS. 1, 2A, 28, 3, 4, 5and 6 . These elements are believed to be self-explanatory and are notdescribed further herein. The precise configuration of the variouscomponents illustrated on these and other Figures do not limit thepresent disclosure.

FIG. 4A is a perspective view of the atomization nozzle 160 with asupport flange 171 according to an embodiment. FIG. 48 is across-sectional view of the atomization nozzle 160 and support flange171 of FIG. 4A. FIGS. 4C, 4D and 4E are top, bottom and perspectiveviews showing details of the atomization nozzle 160 of FIG. 4A,including the central aperture 162 surrounded by radial apertures 166for forming plasma jet channels, for example micro-plasma jet channels.Without limitation, the atomization nozzle 160 may be formed of awater-cooled metal or of a radiation cooled refractory material or acombination of both.

The nozzle 160 is supported by the flange 171. As shown in FIGS. 2A and2B, the flange 171 can be secured between the lower end of the plasmatorch 120 and a mounting annular member 173 in a sealing arrangementbetween the plasma torch 120 and the cooling chamber 170. Stillreferring to FIGS. 2A and 28 , the nozzle 160 comprises an annular,inner surface 177 which may define a portion of the cooling channels 136to provide at the same time for cooling of the nozzle 160. The nozzle160 also defines an annular groove 175 to receive the lower end 211 ofthe plasma confinement tube 179 in a proper sealing arrangement.

The nozzle 160 of FIGS. 4A-4E comprises, on the inner side, a centraltower 168 defining the central aperture 162, which is co-axial with theinjection probe 122. The central aperture 162 has an input funnel-shapedenlargement 169. This configuration of the tower 168 facilitatesalignment and insertion of the forward portion 112 of the feed material110. The central aperture 162 of the nozzle 160 allows the forwardportion 112 of the feed material 110 to exit the plasma torch 120 towardthe inside of the cooling chamber 170.

The atomization nozzle 160 also comprises, around the central tower 168,a bottom wall formed with the plurality of radial apertures 166 equally,angularly spaced apart from each other. The radial apertures 166 aredesigned for allowing respective fractions of the plasma 126 to flowtoward the cooling chamber 170 and generate the plasma jets 180. Thenumber of radial apertures 166 and their angle of attack with respect tothe central, geometrical longitudinal axis of the plasma torch 120 maybe selected as a function of a desired distribution of the plasma jets180 around the longitudinal axis of the plasma torch 120.

The central aperture 162 may be sized and configured to closely match across-section of the feed material 110 so that the central aperture 162becomes substantially closed by insertion of the forward portion 112 ofthe feed material 110 therein. By closing the central aperture 162, apressure of the plasma 126 in the plasma torch 120 builds up. This inturn causes respective fractions of the plasma 126 to be expelled fromthe zone 124 in the plasma confinement tube 179 via the radial apertures166. These expelled fractions of the plasma 126 form the plasma jets180. The radial apertures 166 are sized and configured to expel theplasma jets 180 at high velocity, which could possibly attain sonic orsupersonic velocities.

In cases where the cross-section of the feed material 110 is smallerthan the opening of the central aperture 162, the aperture 162 is notentirely blocked and pressure build-up within the plasma torch 120 maybe of a lesser magnitude. Regardless, the sheer action of the plasmatorch 120 and the partial blockage of the central aperture 162 by thefeed material 110 still cause the plasma 126 to be at a significantpressure level. The plasma jets 180 may still be present, thoughpotentially reduced in terms of flow and pressure. A portion of theplasma 126 is expelled through the central aperture 162, in a gap leftbetween the feed material 110 and the opening of the central aperture162. This portion of the plasma 126 forms an annular plasma jet, orflow, that surrounds the forward end 114 of the feed material 110. As itpasses through the central aperture 162, the forward end 114 can be, insuch cases, atomized in part by the annular plasma jet. The forward end114 may further be atomized in a further part by plasma jets 180 that,though weaker, may still be expelled from the radial apertures 166 ofthe atomization nozzle 160 at a significant speed.

The radial apertures 166 may each be oriented so that the plasma jets180 converge toward the forward end 114 of the feed material 110 in theform of an elongated member such as, as non-limitative examples, a wire,a rod or a filled tube, within the cooling chamber 170 to enhance theatomization process. More particularly. FIGS. 4C and 4D show,respectively, top and bottom views of the atomization nozzle 160. It maybe observed that the radial apertures 166 are angled inwardly about thecentral, geometrical longitudinal axis of the plasma torch 120 from topto bottom of the atomization nozzle 162. In this manner, the plasma jets180 formed therein will converge within the cooling chamber 170 toward aconvergence point in axial alignment with the central aperture 162.Without limitation, the radial apertures 166 may be cylindrical and havea diameter in the range of 0.5 mm up to 3 mm to produce sonic orsupersonic plasma micro-jets and may be oriented at 20° to 70° angleswith respect to the central, geometrical longitudinal axis of the plasmatorch 120. Other shapes and diameters of the radial apertures 166 may ofcourse be contemplated.

As expressed hereinabove, the atomization nozzle 160 generates aplurality of converging plasma jets and may further generate an annularplasma jet. Another embodiment of the atomization nozzle that onlygenerates an annular plasma jet will now be described.

FIG. 5 is a detailed, front elevation view of the plasma torch of FIG. 1, showing an atomization nozzle according to another embodiment. In thisembodiment, the plasma torch 120 is modified to comprise an atomizationnozzle 660 arranged centrally on a bottom closure piece of the torch 120secured to the lower end of the torch body 181. The atomization nozzle660 has a central aperture 662 at its exit end and an internal face 664that tapers off toward the central aperture 662. In a non-limitativeembodiment, the central aperture 662 of the atomization nozzle 660 issized and configured to substantially match a cross-section of theelongated member forming the feed material 110 so moving the forward end114 of the feed material 110 into the atomization nozzle 660 causesbuilding up of a pressure of the plasma 126 in the plasma torch 120. Thepressure of the plasma 126 in the plasma torch 120 causes some of theplasma to be expelled through the atomization nozzle 660, forming anannular plasma jet 665 between the forward end 114 of the feed material110 and the internal face 664 of the atomization nozzle 660. Exposure ofthe forward end 114 of the feed material 110 to the annular plasma jet665 causes surface melting and atomization of the feed material 110. Theatomized feed material exits the plasma torch 120 through the centralaperture 662 and enters the cooling chamber 170 in the form of fine orultrafine droplets 182. The droplets 182 fall into the cooling chamber170, which is sized and configured to allow in-flight freezing of thedroplets 182. The droplets 182, when freezing, turn into powderparticles 184 collected in the collector 190. Some of the plasma,forming the annular plasma jet 665, also enters the cooling chamber 170.

FIG. 6 is a detailed, front elevation view of a variant of the plasmatorch of FIG. 1 , showing the atomization nozzle of FIG. 5 and furtherincluding a sheath gas port surrounding the exit end of the atomizationnozzle. In this variant, the plasma torch 120 of earlier Figures issupplemented by the addition of an input port 410 for receiving a sheathgas 412. The sheath gas 412 is constrained underneath the plasma torch120 by a cover 414 that forms with the bottom closure piece of the torchan annular cavity surrounding the central aperture 662 of theatomization nozzle 560. The sheath gas 412 is expelled from the annularsheath gas output port 416 to form a sheath gas curtain 418 surroundingthe plasma and the droplets 182 expelled from the atomization nozzle660. Presence of the axial sheath gas curtain 418 prevents the droplets182 from reaching and depositing on any downstream surface of the plasmatorch 120, including the atomization nozzle 660. Specifically, thesheath gas curtain 418 prevents rapid expansion of the plasma flowemerging from the atomization nozzle 660 and, therefore, the droplets182 from impinging on any downstream surfaces of the cooling chamber. Asshown on FIG. 6 , the central aperture 662 of the atomization nozzle 660may be extended slightly in a short annular flange 867 to better deflectthe sheath gas 412 around the flow formed by the plasma gas and thedroplets 182. The sheath gas may be of a same nature as the source ofthe plasma gas, including for example inert gases such as argon andhelium to their mixtures with hydrogen, oxygen and/or nitrogen. Thesheath gas may alternatively consist of a different gas.

The apparatus 100 may integrate either of the atomization nozzles 160and 680. Though not illustrated, a further variant of the apparatus 100including a combination of the atomization nozzle 160 with componentsproviding the sheath gas 412 via the sheath gas port 416 is alsocontemplated,

FIG. 7 is a flow chart showing operations of a process of producingpowder particles by atomization of a feed material in the form of anelongated member such as, as non-limitative examples, a wire, rod orfilled tube. On FIG. 7 , a sequence 500 comprises a plurality ofoperations that may be executed in variable order, some of theoperations possibly being executed concurrently, some of the operationsbeing optional.

The sequence 500 for producing powder particles by atomization of a feedmaterial in the form of an elongated member such as, as non-limitativeexamples, a wire, a rod or a filled tube is initiated at operation 510by introducing the feed material in a plasma torch, for example in aninductively coupled plasma torch, introduction of the feed material inthe plasma torch may be made via an injection probe in continuousmanner, using a typical wire, rod or tube feeding mechanism to controlthe feed rate of the elongated member and, if required, to straightenthe elongated member sometimes provided in the form of rolls.

Within the plasma torch, a forward portion of the feed material may bepreheated by either direct or indirect contact with plasma at operation520. When an injection probe is used, a section of the plasma torchbeyond an and of the injection probe, specifically between the end ofthe injection probe and may form a preheating zone for preheating theforward portion of the feed material. Operation 530 comprises moving aforward portion of the feed material from into an atomization nozzle ofthe plasma torch, a forward end of the feed material reaching a centralaperture of the atomization nozzle.

One or more plasma jets are produced by the atomization nozzle. The oneor more plasma jets may include an annular plasma jet surrounding theforward end of the feed material, a plurality of converging plasma jetsexpelled by the atomization nozzle, or a combination of the annular andconverging plasma jets. Generating additional plasma jets using asecondary plasma torch operably connected to the cooling chamber is alsocontemplated. Operation 540 comprises surface melting the forward end ofthe feed material by exposure to the one or more plasma jets formed inthe atomization nozzle.

Droplets formed by atomization of the feed material are frozen in-flightwithin the cooling chamber, at operation 550. Then operation 560comprises collecting powder particles resulting from in-flight freezingof the droplets.

Production of the powder particles using the sequence 500 of FIG. 7 maybe made continuous by continuously advancing the feed material into theplasma torch while maintaining the plasma and plasma jets at propertemperature levels. Generally, a duration of the travel of the forwardportion of the feed material in the preheating zone, whether by directcontact between the feed material and the plasma or indirect radiationheating by the plasma through a radiation tube is controlled so that theforward portion of the feed material reaches a predetermined temperaturebefore moving into the atomization nozzle. The predetermined temperatureobtained in the preheating operation 520 is below a melting point of thefeed material. Control of the duration of the preheating time of thefeed material may be made by controlling a rate of feeding of the feedmaterial and/or a length of the preheating zone in the plasma torch.

Through temperature control of the plasma and of the plasma jets,production of the powder particles using the sequence 500 may apply to abroad range of materials such as pure metals, for example titanium,aluminum, vanadium, molybdenum, copper, alloys of those or other metalsincluding for example titanium alloys, steel and stainless steel, anyother metallic materials having a liquid phase, ceramics including forexample those of oxide, nitride, or carbide families, or any combinationthereof, or any other ceramic material that has a liquid phase,composites or compounds thereof. The foregoing list of materials is notintended to limit the application of the process and apparatus forproducing powder particles by atomization of a feed material in the formof an elongated member.

First Example

According to a first example, the process for producing powder particlesby atomization of a feed material in the form of an elongated member maycomprise the following operations. This first example may make use ofthe apparatus 100 illustrated in whole or in parts in FIG. 1-6 thatincludes the plasma torch 120 for heating, melting and atomizing thefeed material 110. The process involves an axial introduction of thefeed material 110 in the form of an elongated member such as, asnon-limitative examples, a wire, a rod or a filled tube, through theinjection probe 122, into the center of a discharge cavity where theplasma 126 is generated. The feed material 110 may be supplied to theinjection probe 122 in continuous manner by a typical wire, rod or tubefeeding mechanism (not shown) for example similar to commerciallyavailable units currently used in wire arc welding such as the unitscommercialized by Miller for MIG/Wire welding, and comprising, asindicated in the foregoing description, wheels operated to control thefeed rate of the elongated member and, if required, to straighten theelongated member sometimes provided in the form of rolls. As the feedmaterial 110 emerges from the injection probe 122 and traverses theplasma 126, it is heated in the preheating zone 124 before entering intothe downstream atomization nozzle 160 at the lower end of the plasmatorch 120. A distance between the end of the injection probe 122 and theentrance point of the atomization nozzle 160 defines a length of thepreheating zone 124. A time of heating of the feed material 110 by theplasma in the preheating zone 124 depends on the length of thepreheating zone 124 and on a linear speed at which the elongated membertravels in the plasma torch 120. An amount of energy received by thefeed material 110 in the preheating zone 124 depends in turn not only onthe time of preheating of the feed material 110 in the preheating zone126 but also on thermo-physical properties of the plasma 126 as well ason a diameter of the elongated member forming the feed material 110.Through control of the length of the preheating zone 124, the linearspeed of the elongated member forming the feed material 110, and theplasma temperature, it is possible to control the temperature of theforward end 114 of the feed material 110 as it enters into theatomization nozzle 160. For optimal results, the temperature of the feedmaterial 110, as it penetrates into the atomization nozzle 180, may beas high as possible, though preferably not too close to the meltingpoint of the feed material 110 in order to avoid premature melting ofthe feed material 110 in the discharge cavity of the plasma torch 120.

As the preheated forward end 114 of the feed material 110 emerges fromthe atomization nozzle 160 in the cooling chamber 170, it is exposed toa plurality of plasma jets, for example a high velocity, sonic orsupersonic, micro-plasma jets 180 that impinge on the surface of theforward end 114 of the elongated member forming the feed material 110,melts the material and, in statu nascendi, strips out molten material inthe form of finely divided, spherical molten droplets 182 that areentrained by the plasma gas. As the atomized droplets 182 aretransported further downstream into the cooling chamber 170, they cooldown and freeze in-fight forming dense spherical powder particles 184 ofthe feed material. The powder particles 184 are recovered in thecontainer 190 located at the bottom of the cooling chamber 170, or maybe collected in a downstream cyclone (not shown) or collection filter(also not shown), depending on their particle size distribution.

Second Example

Again, this second example may make use of the apparatus 100 thatincludes the plasma torch 120 for heating, melting and atomizing thefeed material 110. According to the second example usable to manufacturepowders of dense spherical particles of metals, metal alloys andceramics, the process for producing powder particles by atomization of afeed material in the form of an elongated member comprises the followingoperations:

a. An inductively coupled plasma source, for example an inductive plasmatorch, comprising a fluid-cooled plasma confinement tube surrounded by afluid-cooled induction coil is provided. The plasma is generated insidethe plasma confinement tube through electromagnetic coupling of theenergy from the induction coil into the discharge cavity in the plasmaconfinement tube. The inductively coupled plasma source operatestypically, without limitation of generality, in a frequency range of 100kHz to 10 MHz with a pressure ranging between soft vacuum of about 10kPa up to 1.0 MPa. The plasma gases can range from inert gases such asargon and helium to their mixtures with hydrogen, oxygen and/ornitrogen. The inductively coupled plasma source comprises a headresponsible for the distribution of a cooling fluid, such as water, thatprovides efficient cooling of all its components. The head may furtherprovide a uniform distribution of a plasma sheath gas into the dischargecavity in order to stabilize the discharge at the center of the tube.The plasma sheath gas also protects the plasma confinement tube fromhigh heat fluxes emanating from the plasma discharge. On a downstreamend of the inductively coupled plasma source, an exit flange-mountednozzle allows the plasma to flow towards a cooling chamber. Theinductively coupled plasma source may also be equipped with a centrallylocated, water-cooled, material injection probe that serves to introducethe material to be processed into the discharge cavity.

b. The feed material to be atomized is introduced through the injectionprobe in the form of an elongated member such as, as non-limitativeexamples, a wire, a rod or a filled tube, in a well-controlled feedrate, using an appropriate feeding mechanism. The feed material may besupplied to the injection probe in continuous manner by a typical wire,rod or tube feeding mechanism (not shown) for example similar tocommercially available units currently used in wire arc welding such asthe units commercialized by Miller for MIG/Wire welding, and comprisingwheels operated to control the feed rate of the elongated member and, ifrequired to straighten the elongated member sometimes provided in theform of rolls.

c. As the feed material to be processed emerges from the injectionprobe, it is directed towards a central aperture in an atomizationnozzle. The presence of the feed material closes at least in part thiscentral aperture of the atomization nozzle.

d. Closing at least in part of the nozzle central aperture causes apressure of the plasma in the discharge cavity to build-up. The pressuremay be in a range of 50 kPa up to 500 kPa or more. This pressure causesa flow of plasma through a plurality of radial apertures in theatomization nozzle, the radial apertures being uniformly distributedover a circular perimeter surrounding the central aperture of thenozzle. This result in the creation of a plurality of focused plasmamicro-jets having a very high speed, possibly reaching sonic orsupersonic values, depending on the configuration and operationalparameters.

e. Exposure of the forward end of the elongated member forming the feedmaterial exits central aperture of the atomization nozzle to penetrate acooling chamber, it is subjected to intense heating by the plasma jets.This completes the melting of the feed material at its surface andatomizes it in the form of fine or ultrafine molten droplets. With thissecond example, droplets having diameters in the range of 5 μm to fewhundred micrometers may be obtained.

f. As the atomized material is entrained in the cooling chamber by theemerging plasma gas, the molten droplets cool down and solidifyin-flight, forming dense spherical particles that are collected at thedownstream part of the system.

Third Example

According to a third example, which may make use of the apparatus 100,the process for producing powder particles by atomization of a feedmaterial in the form of an elongated member comprises the followingoperations.

Feed material 110 in the form of an elongated member such as, asnon-limitative examples, a wire, a rod or a filled tube is introducedthrough the injection probe 122 axially oriented along a centerline ofthe plasma torch 120.

As the feed material 110 emerges from the injection probe 122, at adownstream end of the plasma torch 120, its forward portion 112 isheated either by direct contact with the plasma 126 or indirectly usingthe radiation tube 125 in the preheating zone 124. A distance of travelin the preheating zone 124 and a speed of movement of the feed material110 may be adjusted to allow sufficient time for the forward portion 112of the elongated member to heat to a temperature as close as possible tothe melting point of the feed material, without actually reaching thatmelting point.

At this point, the forward end 114, or tip, of the feed material 110reaches the atomization nozzle 160 and penetrates through its centralaperture 162, which in this third example has substantially the samediameter as that of the elongated member. As the forward end 114 of thefeed material 110 emerges in the cooling chamber 170 from a downstreamside of the atomization nozzle 160, it is exposed to the plurality ofplasma jets 180, for example the high-velocity plasma micro-jets 180impinging thereon. Since the forward end of the feed material 110, beingalready preheated in the preheating zone 124, i.e. in the dischargecavity, to near its melting point, it rapidly melts at its surface andis stripped away by the plasma jets 180, turning into fine or ultrafinedroplets 182 that are entrained by a plasma flow resulting from theplasma jets 180. As the droplets 182 travel down the cooling chamber170, they cool down and solidify in the form of dense sphericalparticles 184 that deposits by gravity in the container 190 at thebottom of the cooling chamber 170 or are transported by the plasma gasto a downstream powder collection cyclone or to a fine metallic filter.

Fourth Example

According to a fourth example, which may make use of the apparatus 100,the process for producing powder particles by atomization of a feedmaterial in the form of an elongated member comprises the followingoperations.

Feed material 110 in the form of an elongated member such as, asnon-limitative examples, a wire, a rod or a filled tube has smallerdiameter than that of the central aperture 162. The feed material 110 isintroduced through the injection probe 122 axially oriented along acenterline of the plasma torch 120.

As in the third example, the feed material 110 emerges from theinjection probe 122, at a downstream end of the plasma torch 120, itsforward portion 112 is heated either by direct contact with the plasma126 or indirectly using the radiation tube 125 in the preheating zone124. A distance of travel in the preheating zone 124 and a speed ofmovement of the feed material 110 may be adjusted to allow sufficienttime for the forward portion 112 of the elongated member to heat to atemperature as close as possible to the melting point of the feedmaterial, without actually reaching that melting point.

At this point, the forward end 114, or tip, of the feed material 110reaches the atomization nozzle 160 and penetrates through its centralaperture 162, which in this fourth example has a larger diameter thanthat of the elongated member. As the forward end 114 of the feedmaterial 110 travels through the central aperture 162 of the atomizationnozzle 160, it is exposed to an annular plasma jet present in a gapformed of a difference between the diameter of the central aperture 162and the diameter of the elongated member. Since the forward end 114 ofthe feed material 110, is already preheated in the preheating zone 124,i.e. in the discharge cavity, to near its melting point, exposition ofthe forward end 114 of the feed material 110 to this annular plasma jetcauses a rapid melting at its surface, being stripped away by theannular plasma jet, turning into fine or ultrafine droplets 182 that areentrained by a plasma flow resulting from the annular plasma jet. If theforward end 114 is not entirely atomized by the annular plasma jet,remaining feed material emerges in the cooling chamber 170 from adownstream side of the atomization nozzle 160. The remaining feedmaterial is exposed to the plurality of plasma jets 180 impingingthereon. The remaining feed material continues melting at its surfaceand, being stripped away by the plasma jets 180, turning into more fineor ultrafine droplets 182 that are entrained by a plasma flow resultingfrom the annular plasma jet and from the plasma jets 180. As thedroplets 182 travel down the cooling chamber 170, they cool down andsolidify in the form of dense spherical particles 184 that deposits bygravity in the container 190 at the bottom of the cooling chamber 170 orare transported by the plasma gas to a downstream powder collectioncyclone or to a fine metallic filter.

An overall view of a typical plasma atomization apparatus 100 is shownin FIG. 3 . The basic dimensions and shapes of the shown components ofthe apparatus 100 may widely vary depending on the material to beatomized and depending on desired production rates. A power level of theplasma torch 120 may, without loss of generality, vary between 10 or 20kW up to hundreds of kW for a commercial production scale unit.

Referring again to FIGS. 4A-4E, an example of design of the atomizationnozzle 160 is shown. The nozzle 160 comprises the flange 171. Theatomization nozzle 180 may be made of fluid-cooled copper or stainlesssteel. Alternatively, the atomization nozzle 160 may be made of arefractory material such as graphite, in combination with a water-cooledflange 171.

The atomization nozzle 160 has a central aperture 162 optionally adaptedto closely match a diameter of the elongated member forming the feedmaterial 110. The atomization nozzle 160 has a plurality of radialapertures 166 equally distributed around the central aperture 162 andwhich, according to an embodiment, are directed at an angle of 45° aboutthe central, geometrical longitudinal axis of the plasma torch 120.Successful operation was obtained using sixteen (16) radial apertures166 having a diameter of 1.6 mm, the radial apertures 166 being equallydistributed around the central aperture 162. The diameter, the numberand the angle of the radial apertures 166 can be adjusted depending onthermo physical properties of the materials to be atomized and on adesired particle size distribution.

It should be pointed out that the atomized material may change itschemical composition during atomization through the reaction betweendifferent components premixed into the feed material. A non-limitativeexample is the production of an alloy by mixing different metals formingthe particles filling a tube forming the feed material. Anothernon-limitative example is a chemical reaction between the chemicalcomponents forming the particles in the filled tube. It should also bepointed out that the atomized material may change its chemicalcomposition during atomization as a result of a chemical reactionbetween the plasma gas(es) and/or sheath gas(es) and the atomizedmaterial, for example by oxidation, nitration, carburization, etc.

Based on fluid dynamic modeling of the flow and temperature field in thedischarge cavity of the plasma torch it is possible to calculate thetemperature profile in the elongated member forming the feed material asit traverses the preheating zone in the torch. FIG. 8 is a schematicview, including a graph showing modelling results for heating a 3.2 mmstainless steel wire introduced in an argon/hydrogen induction plasma at60 kW. FIG. 8 provides typical results that can be obtained using aninductively coupled plasma torch as shown on FIGS. 1-4 . FIG. 8 shows,on its left hand side a two-dimensional temperature field in thedischarge cavity for the argon/hydrogen plasma operated with a radiofrequency power supply with an oscillator frequency of 3 MHz, and aplate power of 60 kW. At the bottom of FIG. 8 , a correspondingtemperature field in a 3.2 mm diameter stainless steel rod is given forrod translation velocities of 40 and 80 mm/s. As expected the overalltemperature of the rod drops with the increase of its translation speedacross the preheating zone in the discharge cavity of the plasma torch.The center of FIG. 8 is a graph showing a variation of the maximumtemperature achieved at the tip of the elongated member, for differentspeeds, and different length of the preheating zone 124, identified onthe left hand side of FIG. 8 as ‘z’. It may be noted that depending onthe length of the preheating zone 124, maintaining the rod translationvelocity within a relatively narrow window allows to avoid the prematuremelting of the material in the discharge cavity or its arrival at theatomization nozzle at too low a temperature, which would have a negativeimpact on the quality of the atomized product.

FIG. 9 is an electron micrograph of powder particles obtained byatomization of a 3.2 mm diameter stainless steel wire and a graph ofcorresponding particle size distribution. Such particles can be obtainedusing the plasma torch of FIGS. 1-6 . Stainless steel powder particleswere obtained using the induction plasma atomization process. The powderparticles had a mean particle diameter, d₅₀ of about 62 μm and thepowder production rate was about 1.7 kg/hour. The powder was mostlycomposed of dense spherical particles. A certain number of splats andsatellites were observed depending on the operating conditions andprocess optimization.

FIG. 10 illustrates electron micrographs of different stainless steelspherical powder fractions produced using the process and apparatus forproducing powder particles by atomization of a feed material in the formof an elongated member. Such particles can be obtained using theinductively coupled plasma torch of FIGS. 1, 2A and 28 . Again, thepowder was mostly composed of dense spherical particles; only few splatsand satellites were observed depending on the operating conditions andprocess optimization.

Those of ordinary skill in the art will realize that the description ofthe process and apparatus for producing powder particles and thedescription of powder particles so produced are illustrative only andare not intended to be in any way limiting. Other embodiments willreadily suggest themselves to such persons with ordinary skill in theart having the benefit of the present disclosure. Furthermore, thedisclosed process, apparatus and powder particles may be customized tooffer valuable solutions to existing needs and problems related toefficiently and economically producing powder particles from a broadrange of feed materials.

Various embodiments of the process for producing powder particles byatomization of a feed material in the form of an elongated member, ofthe apparatus therefor, and of the powder particles so produced, asdisclosed herein, may be envisioned. Such embodiments may comprise aprocess for the production of a broad range of powders including, toughnot limited to, fine and ultrafine powders of high purity metals, alloysand ceramics in an efficient cost effective way that is scalable to anindustrial production level. The process is applicable for theproduction of powders of pure metals, alloys and ceramics, causesminimal or no contamination of the atomized material, causes minimal orno oxygen pickup especially for reactive metals and alloys, producesfine or ultrafine particle size, for example with particle diameter lessthan 250 μm, the particles being dense and spherical, with minimal or nocontamination with satellites.

In the interest of clarity, not all of the routine features of theimplementations of process, apparatus, and use thereof to produce powderparticles am shown and described. It will, of course, be appreciatedthat in the development of any such actual implementation of theprocess, apparatus, and use thereof to produce powder particles,numerous implementation-specific decisions may need to be made in orderto achieve the developer's specific goals, such as compliance withapplication-, system-, and business-related constraints, and that thesespecific goals will vary from one implementation to another and from onedeveloper to another. Moreover, it will be appreciated that adevelopment effort might be complex and time-consuming, but wouldnevertheless be a routine undertaking of engineering for those ofordinary skill in the field of materials processing having the benefitof the present disclosure.

Although the present disclosure has been described hereinabove by way ofnon-restrictive, illustrative embodiments thereof, these embodiments maybe modified at will within the scope of the appended claims withoutdeparting from the spirit and nature of the present disclosure.

1-50. (canceled)
 51. A process to produce powder from a feed material inthe form of an elongated member by plasma atomization, comprising:preheating the feed material using a device for preheating the feedmaterial, wherein the device for preheating the feed material includesan induction coil; atomizing the feed material in an atomization zonewith at least one plasma jet; and cooling atomized particles to solidstate to produce the powder.
 52. The process of claim 51, wherein theinduction coil is configured to generate energy to preheat the feedmaterial.
 53. The process of claim 52, wherein the induction coil isconfigured to generate plasma forming the at least one plasma jet. 54.The process of claim 52, wherein the device for preheating the feedmaterial transfers heat to the feed material in a contactless manner.55. The process of claim 51, wherein the feed material comprises a puremetal, an alloy, a ceramic, or a composite material.
 56. The process ofclaim 55, wherein the elongated member is a rod, a wire, or a filledtube.
 57. The process of claim 51, wherein the cooling the atomizedparticles is performed in a cooling chamber, the process furthercomprising collecting the powder downstream from the cooling chamber ina powder collector.
 58. The process of claim 57, wherein the powdercollector includes a cyclone.
 59. The process of claim 51, wherein thedevice for preheating the feed material includes a tubular structureconfigured to transfer heat to the feed material.
 60. The process ofclaim 59, wherein the tubular structure is made of refractory material.61. The process of claim 60, wherein the tubular structure includes aradiation tube.
 62. The process of claim 61, wherein the radiation tubeheats the wire through radiation.
 63. The process of claim 60, whereinthe refractory material includes graphite, tungsten or hafnium carbide.64. The process of claim 51, wherein the preheating includes exposing asurface of a forward portion of the elongated member to direct contactwith plasma produced with the induction coil to pre-heat the feedmaterial of the forward portion.
 65. The process of claim 51, whereinthe at least one plasma jet includes a plurality of plasma jetsimpinging on the feed material at an impingement point in theatomization zone for causing progressive melting of the feed materialand breakdown into atomized particles.
 66. The process of claim 51,wherein the at least one plasma jet is generated from a gas comprisingargon, helium, or a combination thereof.
 67. The process of claim 66,wherein the gas further comprises oxygen, hydrogen, or nitrogen.
 68. Theprocess of claim 51, wherein the preheating is performed over a segmentof the elongated member, the segment having a length of from about 10 mmto about 125 mm.
 69. The process of claim 51, wherein the elongatedmember is fed to the atomization zone at a material feed rate of fromabout 4.5 kg/h to about 11.2 kg/h.
 70. The process of claim 51, whereinplasma of the at least one plasma jet is generated with a power levelabove 10 kW.
 71. The process of claim 51, wherein the preheating isperformed to a near-melting temperature that is within 500K of themelting point of the feed material.
 72. The process of claim 51, whereinthe at least one plasma jet includes an annular plasma, a plurality ofplasma jets, or a combination thereof.
 73. The process of claim 71,wherein each plasma jet of the plurality of plasma jets is oriented from20 degrees to 70 degrees with respect to a longitudinal axis of the feedmaterial at the atomization zone.
 74. The process of claim 51, furthercomprising providing a feeding mechanism configured to feed theelongated member to the atomization zone.
 75. The process of claim 74,wherein the elongated member is fed from a roll of the feed material,wherein the feeding mechanism is further configured to straighten theelongated member.
 76. The process of claim 75, wherein the elongatedmember is a wire and the feeding mechanism includes straightening wheelsto straighten the wire being fed from the roll of the feed material. 77.The process of claim 74, wherein the feeding mechanism is furtherconfigured to control a feed rate of the feed material.